Two-Dimensional Thin-Layer Chromatography of Selected Coumarins (original) (raw)
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Jpc – Journal Of Planar Chromatography – Modern Tlc, 2008
Polar-bonded stationary phases (CN-silica and Diol-silica) are used with nonaqueous eluents in adsorption mode or with aqueous eluents in partition mode. This enables the application of these systems in two-dimensional separations because of the different selectivity and application to the separation of closely related compounds of similar physicochemical properties and retention behaviour. Similarly, multiphase plates, connected with C18 strips and silica layers, are used with aqueous and nonaqueous eluents. Such layers were applied for the separation of selected coumarins. Thus, differences in separation selectivity are applied for the separation of coumarin fractions from plant extracts of the Apiaceae family by two-dimensional thin-layer chromatography.
Jpc – Journal Of Planar Chromatography – Modern Tlc, 2008
Polar-bonded stationary phases (CN-silica and Diol-silica) are used with nonaqueous eluents in adsorption mode or with aqueous eluents in partition mode. This enables the application of these systems in two-dimensional separations because of the different selectivity and application to the separation of closely related compounds of similar physicochemical properties and retention behaviour. Similarly, multiphase plates, connected with C18 strips and silica layers, are used with aqueous and nonaqueous eluents. Such layers were applied for the separation of selected coumarins. Thus, differences in separation selectivity are applied for the separation of coumarin fractions from plant extracts of the Apiaceae family by two-dimensional thin-layer chromatography.
Thin-layer chromatography of some coumarin derivatives
Journal of Chromatography A, 1976
Suitable methods for the separation and identification of 4hydroxycoumarin derivatives are desirable in view of the physiofogical activities of these compounds, and their usefulness in therapy. Paper and thin-layer chromato,gaphy (PC and TLC) have already been used in the examination of various anticoagulant dicoumarok', of some coumarin derivatives with rodenticidalz*3, bactericidal and fungicidal activities and of several further types of coumarin derivatives of potential importancC*'.
Purification of Coumarin Compounds From Cortex fraxinus by Adsorption Chromatography
Journal of Chromatographic Science, 2013
In this paper, a chromatographic method for isolation and purification of coumarin compounds from Cortex fraxinus was established by using Superose 12 as the separation media for the first time. The conditions for separation were optimized. Four kinds of coumarin compounds including aesuletin, aesculin, fraxetin and fraxin were obtained. The purity of these compounds were 98.5, 99.1, 97.9 and 97.3%, respectively, which were determined by HPLC area normalization method. The chemical structures of the separated compounds were identified according to 1 H and 13 C nuclear magnetic resonance data. The retention behavior of the separated coumarin compounds on Superose 12 was also discussed. The retention is based on a mixture of hydrogen bonding and hydrophobic interactions between the coumarin compounds and the residues of the cross-linking reagents used in the manufacturing process of Superose 12. The results of this paper indicate that Superose 12 is not only suitable for size-exclusion chromatography of proteins and other biological macromolecules but also for low-molecular-weight natural products.
HPLC-MS and MECC analysis of coumarins
Chromatographia, 1997
MECC separation of 11 coumarins has been achieved by use of a running electrolyte at pH 10.4 prepared from 50 mM boric acid, 10 mM sodium tetraborate and 100 mM sodium hydroxide. The buffer solution contained 50 mM SDS and, as organic modifier, 1% n-propanol. The applied voltage was 25 kV and the temperature of the capillary was kept constant at 20 ~ HPLC baseline separation of the coumarin mixture was obtained by use of a reversed-phase column and an acetonitrile-water solvent gradient. UV detection was performed at 205 nm. Peak assignment and purity control were achieved by HPLC-mass spectrometry with either an electrospray interface or an atmospheric-pressure chemical-ionization interface. Compounds were detected in either negative-or positive-ion modes. These MECC and HPLC-MS methods are suitable for 'fingerprint' analysis of a number of coumarin-containing plants, e.g. Fr. Ammi visnagae, Rd. Scopoliae and Rd. Imperatoriae.
Journal of Separation Science, 2003
HPLC-DAD in identification and quantification of selected coumarins in crude extracts from plant cultures of Ammi majus and Ruta graveolens This paper describes a method for the separation and determination of selected coumarins and furanocoumarins in the crude extracts from plant tissue cultures of Ammi majus hairy roots and Ruta graveolens cell suspensions, cultured in vitro, separately or together as co-cultures. The usefulness of the three main components of the eluent used in reversed-phase high performance liquid chromatographic analysis, namely: methanol (MeOH), acetonitrile (ACN), and tetrahydrofuran (THF), and different elution programs, was assessed. In the optimal analytical method a Lichrospherm RP-18e 5-lm column, a THF-MeOH elution gradient, and a UV/VIS DAD detector were used. Due to the presence of many different compounds in the investigated plant extracts, the use of a UV/VIS DAD detector was essential. Coumarins were identified by comparison of their UV spectra with those of the analytical standards, and characterization of peak purity.
Journal of the American …, 1995
Coumarins are a large group of compounds that are naturally present in plant tissues and that exhibit a wide range of pharmacological properties. Analytical methods based on chromatographic techniques and conventional detectors are inadequate to accurately analyze coumarins in complex matrices such as plant extracts. In this article a new method based on a modified particle beam liquid chromatography-mass spectrometry interface is described. The method allows specific and accurate determination of several coumarins in biological matrices. An application regarding the analysis of 18 coumarins in the extract of Smyrnium perfoliatum L. is also reported.
JPC - Journal of Planar Chromatography - Modern TLC, 2005
Preparative separation and isolation of coumarins from petroleum ether and methanol extracts of the fruits and roots of Peucedanum verticillare L. Koch ex DC (Umbelliferae = Apiaceae) have been achieved by column chromatography and normal-and reversedphase TLC with gradient elution. Isolated coumarins were identified by comparison with standards in analytical TLC and in RP HPLC with gradient elution, by melting point (m.p.) measurement, by UV spectroscopy, by MS, and by 1 H and 13 C NMR spectroscopy. Esculin, umbeliferone, bergapten, xanthotoxin, isoimperatorin, imperatorin, psoralen, and cis-kellactone were isolated for the first time from P. verticillare L. Koch ex DC. Two angular-type pyranocoumarins isolated from the roots and fruits of Peucedanum verticillare L. Koch ex DC. were identified as pteryxin and epoxypteryxin by MS and 1 H and 13 C NMR.
Annals of Advances in Chemistry, 2021
A micellar thin-layer chromatography method for the quantitative determination and validation of coumarin in Meliloti herba and its ethanolic extracts was developed and validated. For achieving good determination, the mobile phase of 5 x 10-4 mol/L Tween-80 in a mixture propanol-2 – water (5:95 v/v) was used. Densitometric determination was carried out at 275 nm. The calibration curve was linear in the range of 0.1-2.5 μg per band. The proposed method is simple, rapid, precise and accurate; replacing hazardous solvents by greener ones correspond to the modern requirements in “Green chemistry” concepts. The obtained data can be used for the routine analysis of coumarin in medical plant and extracts.
Spray reagent for the detection of coumarins and flavonoids on thin-layer plates
Journal of Chromatography A, 1987
Thin-layer chromatography (TLC) has already proved its worth in the dewtion of various types of chemical compounds having different structures. Its wide application to natural product chemistry is of prime importance. In TLC, spray reagents have been successfully utilized for detection of oxygen heterocycles, viz., coumarins and flavonoids. The most effective reagent for the detection of coumarins is methanolic potassium hydroxider; diazotized sulphanilic acid2 is also well established for this purpose. The Lewis acids, e.g., aluminium chloride3 and antimony(III) chloride*, basic lead acetate4, p-toluenesulphonic acid5 and iodine-potassium iodide6 are well documented for the detection of flavonoids. Benedict's reagent7 has been used for the simultaneous detection of coumarins and flavonoids in TLC, Chalconcss can be detected by spraying sulphuric acid-ferric chloride followed by irradiation of the spots with short-wavelength UV light.